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WO2018041488A1 - Procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires - Google Patents

Procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires Download PDF

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Publication number
WO2018041488A1
WO2018041488A1 PCT/EP2017/069032 EP2017069032W WO2018041488A1 WO 2018041488 A1 WO2018041488 A1 WO 2018041488A1 EP 2017069032 W EP2017069032 W EP 2017069032W WO 2018041488 A1 WO2018041488 A1 WO 2018041488A1
Authority
WO
WIPO (PCT)
Prior art keywords
removal
product
hemicelluloses
isolation
suspended solids
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2017/069032
Other languages
English (en)
Inventor
Oleg Shagaev
Lukas WIESEGGER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Andritz AG
Original Assignee
Andritz AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Andritz AG filed Critical Andritz AG
Priority to US16/326,769 priority Critical patent/US10870947B2/en
Priority to CN201780053705.1A priority patent/CN109642394B/zh
Priority to EP17748707.1A priority patent/EP3507415B1/fr
Priority to CA3035614A priority patent/CA3035614C/fr
Priority to JP2019512192A priority patent/JP6752359B2/ja
Priority to NZ750018A priority patent/NZ750018B2/en
Priority to RU2019106210A priority patent/RU2713239C1/ru
Priority to AU2017318207A priority patent/AU2017318207B2/en
Priority to BR112019001781-0A priority patent/BR112019001781B1/pt
Publication of WO2018041488A1 publication Critical patent/WO2018041488A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0007—Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0042—Fractionating or concentration of spent liquors by special methods
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0085—Introduction of auxiliary substances into the regenerating system in order to improve the performance of certain steps of the latter, the presence of these substances being confined to the regeneration cycle
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/04—Regeneration of pulp liquors or effluent waste waters of alkali lye
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/10—Concentrating spent liquor by evaporation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the invention relates to a process for isolation of hemicelluloses from biomass pulping process waters and spent liquors with removal of suspended solids, concentration of the product and purification of the product by removal of inorganic salts and low molecular weight substances.
  • hemicelluloses e.g. xylooligosaccharides (XOS)
  • XOS xylooligosaccharides
  • PHA polylactic acid
  • concentration of the effluent the throughput (flux) was very low in ultrafiltration process. So approx. 1 - 3% solids content could be achieved with a throughput of only 10 - 15 l/m 2 h, or less by the time this concentration could be reached.
  • PFA polylactic acid
  • Such low throughput is mainly due to fouling of the ultrafiltration units.
  • the invention is characterized in that the hemicellulose isolation process conditions at several separation/purification stages are adjusted separately by e.g. pH
  • An advantageous embodiment of the invention is characterized in that the pH value of the incoming effluent stream is adjusted to pH 8 - 11. With such measure a good separation of fibers, suspended solids and hemicelluloses is possible.
  • a further improvement of the invention is characterized in that pH value of the clear fluid stream after the removal of the coarse suspended solids is adjusted to pH 8-11 , preferably pH 9.0 - 9.5. With this adjustment the fouling of filter surfaces, especially membranes, is reduced significantly.
  • a further development of the invention is characterized in that before removal of inorganic salts the pH value is adjusted to 4.0 - 4.5. Such pH adjustment allows that no sodium ions are bound to the hemicelluloses and thus can be separated easily.
  • An advantageous improvement of the invention is characterized in that the final product enriched with hemicellulose after separation of ashes has a dryness of 15- 30%. This allows cheaper thermal isolation treatment afterwards.
  • the invention further relates to a plant for isolation of hemicelluloses from biomass pulping process waters or spent liquors with units for removal of suspended solids, concentration of the product and purification of the product by removal of inorganic salts and low molecular weight substances.
  • This is characterized in that a line for adding chemicals to adjust the pH value is provided at several separation/purification units.
  • concentrations and the optimal pH value for separation and purification can be set.
  • the units for separation of suspended solids are mechanical separation units as e.g. centrifuges, filters or the like. So the main portion of fibers can be separated and possibly reused easily.
  • a further development of the invention is characterized in that as concentration unit membrane filters are provided. These filters can separate the suspended solids at a high ratio.
  • An advantageous improvement of the invention is characterized that as purification unit for e.g. ash removal membrane filters are provided the corresponding product purity can be achieved according to the desired level.
  • a further improvement of the invention is characterized in that a thermal separation unit is provided to concentrate the product. Depending on the demands the product can be sold and transported with a little portion of water only.
  • FIG. 1 shows the typical setup of the preferred process.
  • This process for isolation of hemicelluloses can be used for mechanical pulping lines, semi-chemical and chemical pulping plants. It can be implemented in either existing installations or rebuild projects.
  • the process applies for biomass, hardwood (xylans) and softwoods (galactoglucomannans (GGM)) pulping lines process waters and spent liquors treatment where alkaline treatment or high temperature water extraction of biomass is used.
  • Typical pulping lines for isolation of hemicelluloses from process waters, bleach plants and spent liquors are:
  • the incoming stream A in Fig. 1 can be any effluent of any mechanical or semi- chemical pulping line containing hemicellulose, which can be e.g. white water or pressate, or filtrate, or black liquor from pulp washing equipment normally at a temperature of e.g. 60 - 90°C.
  • the incoming stream A loaded with a high amount of COD (chemical oxygen demand) as "effluent" is usually sent to an effluent treatment station, which is the current state-of-the-art.
  • COD chemical oxygen demand
  • the pH is adjusted to pH 8-11 by stream B.
  • first pH adjustment - stream C - containing coarse suspended solids such as fibers and fiber particles and particles greater than > 10 pm that are not retained during washing are removed in the first process step I, whereby some separation equipment allows to remove particles greater than > 5 pm.
  • Process step I can be performed by mechanical separation equipment such as filtration units or centrifuges (e.g. decanter centrifuge).
  • the necessity to use for example a decanter centrifuge is suitable for the APMP lines without existing fiber recovery system (e.g. fiber recovery disc filter) that is capable to remove fiber fragments, fines and other suspended solids from screw press pressate after an alkaline peroxide bleaching stage.
  • the decanter centrifuge is used to remove suspended solids.
  • existing fiber recovery system e.g. having the fiber recovery disc filter
  • fiber recovery disc filter that is capable to remove efficiently fiber fragments, fines and other suspended solids from pulp washing equipment
  • the clear fluid (stream G) from coarse suspended solids removed in process step I e.g. either by a disc filter or decanter centrifuge, the effluent is collected in a buffer tank where the pH value of this spent liquor is adjusted to pH 8-11 (more
  • stream H - advantageously to pH 9.0-9.5) by stream H - to dissolve the high molecular weight hemicelluloses, that tend to coagulate and/or absorb on high specific surface fines/particles at pH ⁇ 6-7 after a neutralization stage that is typically performed after the bleaching stage in APMP/BCTMP processes.
  • adjustment of the pH value may only be done with adding the basic chemicals in stream B, in other applications chemical addition to get to pH 8 - 11 , preferably 9.0 - 9.5, can be done in stream H.
  • this fraction is transferred to the liquid phase of the effluent - stream I - and is sent to process step II, where smaller particles in the range of > 0.5 - 10 pm are removed, e.g. very fine biomass material and colloidal suspended solids (e.g. silicates, resins).
  • colloidal suspended solids e.g. silicates, resins
  • machines and equipment such as centrifugal disc separators (or other type of separators), or membrane type micro filtration units can be used.
  • the effluent J is sent to process step III, in which the hemicelluloses are enriched.
  • the reject streams of process step I - stream D- and of process step II - stream E, containing fibers and other suspended solids down to approx. 0.5 pm particle size, are collected and can be sent back to the system (mechanical or semi-chemical pulping line or pulp and paper mill) - stream F.
  • process step III usually ultrafiltration membrane units are used and most of the water, salts and low molecular organics are removed and the effluent/product is concentrated to a factor of 10-20.
  • the permeate of this process step - stream K - having much less COD (chemical oxygen demand) than stream A thus can be reused in the system (mechanical or semi-chemical pulping line or pulp and paper mill).
  • the pH of the concentrated liquor / effluent L is adjusted by stream M and the resulting stream N is passing through the next process step IV, which is a membrane unit - usually diafiltration, where stream N is washed by fresh water or process condensate - stream P and inorganic salts (mostly sodium) are removed to the required product quality level and the product is concentrated further to the level of solids content sufficient for the next process step(s).
  • the pH of stream L is adjusted to pH 4.0-4.5 by acid, e.g. sulfuric acid, hydrochloric acid etc. by stream M in order to have more efficient removal of bound sodium ions (Na + ) and, correspondingly, reduce the product ash content further if required.
  • Process step IV is able to produce the product (stream Q) at 20-30% solids concentration.
  • Process step IV generates excess water / permeate O, which can be used for dilution or any further use in the system (mechanical or semi-chemical pulping line or pulp and paper mill) to substitute fresh water or any mill water.
  • the out coming stream Q of process step IV is further processed in process step V, where the hemicelluloses are thickened further up to a solid concentration of 50 - 80 %.
  • the invention is not limited to the drawing but the process may also already end after process step IV when the stream may be further used in the system. Also excess water (stream R) of process step V may be reused instead of fresh water for stream P of process step IV.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Sustainable Development (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Molecular Biology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Paper (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne un procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires avec élimination de solides en suspension, concentration du produit et purification du produit par élimination de sels inorganiques et de substances à faible poids moléculaire. L'invention est caractérisée en ce que les conditions de procédé d'isolation d'hémicellulose lors de plusieurs étapes de séparation/purification sont ajustées séparément, par exemple un ajustement de pH. La présente invention concerne en outre une installation destinée à exécuter le procédé. Avec ledit procédé et ladite installation, il est possible de récupérer la plupart des matières en suspension, en particulier le xylane et d'autres hémicelluloses.
PCT/EP2017/069032 2016-09-02 2017-07-27 Procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires Ceased WO2018041488A1 (fr)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US16/326,769 US10870947B2 (en) 2016-09-02 2017-07-27 Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors
CN201780053705.1A CN109642394B (zh) 2016-09-02 2017-07-27 从生物质制浆工艺水或废液中分离出半纤维素的方法
EP17748707.1A EP3507415B1 (fr) 2016-09-02 2017-07-27 Procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires
CA3035614A CA3035614C (fr) 2016-09-02 2017-07-27 Procede d'isolation d'hemicelluloses a partir d'eaux de procede de reduction en pate de biomasse ou de liqueurs residuaires
JP2019512192A JP6752359B2 (ja) 2016-09-02 2017-07-27 バイオマス・パルプ化のプロセス水または廃液からヘミセルロースを単離する方法
NZ750018A NZ750018B2 (en) 2017-07-27 Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors
RU2019106210A RU2713239C1 (ru) 2016-09-02 2017-07-27 Способ выделения гемицеллюлоз из технологических вод процесса преобразования биомассы в волокнистую массу или отработанных щелоков
AU2017318207A AU2017318207B2 (en) 2016-09-02 2017-07-27 Process for isolation of hemicelluloses from biomass pulping process waters or spent liquors
BR112019001781-0A BR112019001781B1 (pt) 2016-09-02 2017-07-27 Processo para isolamento de hemiceluloses de águas de processos de polpação de biomassa ou soluções esgotadas

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ATA50780/2016 2016-09-02
ATA50780/2016A AT519059B1 (de) 2016-09-02 2016-09-02 Verfahren zur Abtrennung von Hemizellulosen aus Biomasse-Aufschlussprozesswasser oder verbrauchten Laugen

Publications (1)

Publication Number Publication Date
WO2018041488A1 true WO2018041488A1 (fr) 2018-03-08

Family

ID=59523096

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2017/069032 Ceased WO2018041488A1 (fr) 2016-09-02 2017-07-27 Procédé d'isolation d'hémicelluloses à partir d'eaux de procédé de réduction en pâte de biomasse ou de liqueurs résiduaires

Country Status (11)

Country Link
US (1) US10870947B2 (fr)
EP (1) EP3507415B1 (fr)
JP (1) JP6752359B2 (fr)
CN (1) CN109642394B (fr)
AT (1) AT519059B1 (fr)
AU (1) AU2017318207B2 (fr)
BR (1) BR112019001781B1 (fr)
CA (1) CA3035614C (fr)
CL (1) CL2019000545A1 (fr)
RU (1) RU2713239C1 (fr)
WO (1) WO2018041488A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111961695B (zh) * 2020-07-02 2022-07-29 上海昶法新材料有限公司 利用溶解浆预蒸煮废液制备低聚糖的方法
CN111943994B (zh) * 2020-07-02 2022-02-01 上海昶法新材料有限公司 利用溶解浆预蒸煮废液制备木糖的方法

Citations (5)

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US4470876A (en) * 1982-07-22 1984-09-11 Beaupre Marc F Kraft overload recovery process
WO2002040767A1 (fr) * 2000-11-16 2002-05-23 Raisio Chemicals Ltd Procede de recuperation de substances non fibreuses a partir de materiaux de bois
WO2004013409A1 (fr) * 2002-07-25 2004-02-12 Coffin World Water Systems Appareil et procede de traitement de liqueur noire
US20120196233A1 (en) * 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20140163245A1 (en) * 2011-05-26 2014-06-12 Michael A. Lake Process for producing furfural from black liquor

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AT413697B (de) * 2001-11-07 2006-05-15 Andritz Ag Maschf Verfahren zur behandlung säurehältiger abwässer
US7101996B2 (en) * 2003-09-23 2006-09-05 Corn Products International, Inc. Process for preparing purified fractions of hemicellulose and cellulose-hemicellulose complexes from alkali treated fiber and products made by the process
FI120045B (fi) * 2005-12-22 2009-06-15 Roal Oy Selluloosamateriaalin käsittely ja siinä käyttökelpoiset entsyymit
JP2011019489A (ja) * 2009-07-21 2011-02-03 Hbi Kk 水溶性ヘミセルロースの調製方法
CN102838693A (zh) * 2011-06-21 2012-12-26 北京林业大学 从生物质中分离纯化直链半纤维素和支链半纤维素的方法
US20130115653A1 (en) * 2011-11-09 2013-05-09 Thesis Chemistry, Llc Method for producing biobased chemicals from woody biomass
SE1551720A1 (sv) * 2013-05-29 2015-12-29 Kiram Ab A method for the treatment of spent pulping liquor for the removal and production of a ligning containing product
CN103541260A (zh) * 2013-10-28 2014-01-29 宜宾海丝特纤维有限责任公司 一种从制浆黑液中回收半纤维素的方法
US10145063B2 (en) * 2014-08-29 2018-12-04 University Of Tennessee Research Foundation Comprehensive process for selectively separating lignocellulosic biomass into purified components with high yield
CN104558632B (zh) * 2014-12-30 2017-01-11 山东龙力生物科技股份有限公司 一种利用工业纤维废渣制备木质素衍生产品的方法
US11154087B2 (en) * 2016-02-02 2021-10-26 R.J. Reynolds Tobacco Company Method for preparing flavorful compounds isolated from black liquor and products incorporating the flavorful compounds
CN105714590B (zh) * 2016-04-15 2017-10-31 广西科学院 从造纸黑液中分离木质素和半纤维素并回收碱液的方法
DE102016219719B3 (de) * 2016-10-11 2018-01-25 Clariant International Ltd. Verfahren zur Gewinnung von Cellulose, Hemicellulose und Lignin aus Lignocellulose aus pflanzlicher Biomasse

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4470876A (en) * 1982-07-22 1984-09-11 Beaupre Marc F Kraft overload recovery process
WO2002040767A1 (fr) * 2000-11-16 2002-05-23 Raisio Chemicals Ltd Procede de recuperation de substances non fibreuses a partir de materiaux de bois
WO2004013409A1 (fr) * 2002-07-25 2004-02-12 Coffin World Water Systems Appareil et procede de traitement de liqueur noire
US20120196233A1 (en) * 2011-02-01 2012-08-02 Yonghao Ni Recovery of dissolved organics from lignocellulosic solutions
US20140163245A1 (en) * 2011-05-26 2014-06-12 Michael A. Lake Process for producing furfural from black liquor

Also Published As

Publication number Publication date
AT519059B1 (de) 2018-07-15
EP3507415B1 (fr) 2020-04-01
AU2017318207A1 (en) 2019-02-07
BR112019001781A2 (pt) 2019-05-07
CA3035614A1 (fr) 2018-03-08
US20190203416A1 (en) 2019-07-04
US10870947B2 (en) 2020-12-22
EP3507415A1 (fr) 2019-07-10
CL2019000545A1 (es) 2019-05-31
CN109642394A (zh) 2019-04-16
AU2017318207B2 (en) 2021-07-08
JP6752359B2 (ja) 2020-09-09
NZ750018A (en) 2024-08-30
AT519059A1 (de) 2018-03-15
RU2713239C1 (ru) 2020-02-04
CN109642394B (zh) 2021-07-30
BR112019001781B1 (pt) 2023-04-11
CA3035614C (fr) 2023-05-16
JP2019529612A (ja) 2019-10-17

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